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By R. A. Stauffer

THE chief ore of lithium is spodumene, a lithium-aluminum silicate containing up to 3 pct lithium. The preparation of lithium salts from spodumene is costly because of the low concentration of the metal and the difficulty of separating it from the other alkali metals present. Dr. Kroll's and Dr. Schlecten's recent paper' has reviewed various methods proposed for preparation of lithium. It will be seen from this paper that the methods proposed to date have required one or another of the lithium salts as a raw material. The high cost of these salts has been the chief item of expense in the lithium metal produced. This situation has made it interesting to investigate the possibility of producing the metal directly from spodumene. When spodumene is calcined at 1000°C in the presence of lime, lithium oxide is replaced in the ore as is evidenced by the fact that it may be leached from the reaction mixture with water.2 Free energy calculations suggested that lithium oxide might be reduced with aluminum or silicon and the lithium produced distilled from the reaction mixture by heating to about 1000°C in a vacuum. These facts taken together suggested that it might be possible to prepare lithium metal directly from spodumene by heating a mixture of the ore, lime, and a suitable reducing agent in vacuum and distilling off the lithium metal as formed. THE REPLACEMENT OF Li20 IN SPODUMENE A series of experiments were undertaken to determine the ratio of lime to spodumene necessary to free substantially all the lithium oxide present in the ore. The spodumene used in these experiments was supplied by Foote Mineral Co. in the form of powder of about 200 mesh. Analysis of the spodumene was as follows: [ ] Lime (cp -200 mesh) was added in various ratios to spodumene and thoroughly mixed in a ball mill. Two hundred gram samples of spodumene-lime mixtures were charged loosely in fireclay crucibles and held at 1000°C in a gas-fired furnace for 5 hrs. The product in each case was ground to pass 140 mesh and then placed in a thimble in a soxhlet extractor. Extraction with water was carried on for 6 hrs. After this period the extract was reduced in volume by evaporation in order to precipitate dissolved lime and was then filtered and titrated with 1/4 normal hydrochloric acid. After correcting for residual calcium oxide in solution, the alkali present was calculated as lithium oxide. The results of these experiments are shown in Table I and Fig I. At lime-spodumene ratios less than 1.5, the products were invariably fused. At the ratio of 1.5 and above, the product was loosely sintered with little evidence of fusion. When the ratio of lime to spodumene was three, replacement of alkali oxides in the

Jan 1, 1947

By M. C. Flemings, R. Mehrabian, G. E. Nereo

Analytical expressions derived previously are used to describe quantitatively effects on macrosegregation of some solidification and mold design variables. Al-4.5 pct Cu alloy is used as example. It is shown that abrupt changes in heat transfer rate result in solute-rich or solute-poor "bands". Severe solute-rich bands accowzpany "reheating" that can result, for example, from abrupt formation of an air gap at a mold-metal interface. With planar isotherms, solute-poor regions also result from reduction in cross section through which fluid flow to feed shrinkage takes place. It is suggested that the negative "cone" of segregation often found at the base of large ingots results from this reduction in cross section for feeding. Consideration is given to the positive and negative segregation to be expected in laboratory ingots in association with changes in ingot cross section. Under-riser positive segregation is considered and it is concluded this segregation results when vertical temperature gradient is low in the region of the riser; the segregation is accentuated by the temperature gradient reversal which can occur in inadequately insulated risers ("'hot tops"). Finally it is shown for Al-4.5 pct Cu alloy that the assumption of constant k and p in analytic solutions gives calculated results close to those obtained for the case of ziariable k and 0. A basic "local solute redistribution equation" was derived earlier' for calculation of macrosegregation resulting from flow of solute-rich liquid to feed solidification shrinkage, thermal contraction, and/or other contractions occurring during solidification. This expression relates fraction liquid, g~, to liquid composition, CL, at a given position x, y, z, in a solidifying Eq. [I] is for the general case of three-dimensional heat and fluid flow assuming constant solid (but not necessarily liquid) density during solidification, negligible net solute change from diffusion, and no pore formation. In this paper we first demonstrate application of this equation for calculation of macrosegregation in several examples involving one-dimensional heat and fluid flow. Specifically considered are examples in which segregation results from sudden changes in heat flow conditions. Next, Eq. [I] is used to describe segregation in examples where isotherms remain planar but where fluid flow is no longer one-dimensional. Application of this expression illustrates the type of segregation to be expected in unidirectionally solidified ingots of gradually or abruptly varying cross section. For segregation calculations, A1-4.5 pct Cu alloy is employed with constant k and p Vz = 0.172, 4 = 0.055), eutectic composition (CE = 33 pct Cu). In all examples, fraction eutectic is neglected in velocity calculations; this was previously shown to introduce little error.' A linear distribution of fraction liquid in the liquid-solid zone is assumed. In a concluding section it is shown that the assumption employed of constant k and /3 gives results close to those obtained when the actual (variable) values of k and 0 are employed.

Jan 1, 1969

By D. J. Jr. McAdam

PART I. OUTLINE OF INVESTIGATION, DESCRIPTION OF MATERIAL AND METHODS RESULTS of investigation of corrosion-fatigue of metals at the U. S. Naval Engineering Experiment Station, Annapolis, Md., have been discussed by the writer in several recent papers.1,2,3,4 In those papers references were also given to the work of Haigh in 1917.6 Efforts by the writer to obtain a better understanding of some of the factors involved in corrosion-fatigue finally developed into a general investigation of the effect of time and cyclic stress on corrosion of metals. Corrosion fatigue of Metals As described in the papers mentioned, rotating-cantilever specimens, conically tapered so that the stress is nearly uniform over a length of about 1.5 in., were subjected to simultaneous fatigue and corrosion. For this purpose a stream of water was diagonally applied so as to sweep the specimen from the outer to the inner fillet and surround the stressed surface with water. The fresh water is a calcium carbonate water, the composition of which has been given in a previous paper.2 The salt water is Severn River water having a saline content about one-third that of sea water.

Jan 1, 1928

By W. L. Phillips

Nickel alloys containing approximately 0.5, 2.0, and 6.0 at. pct of Os, Pd, Ru, and Rh were Prepared by vacuum melting. Tension tests were carried out at 25°, 500°, 800°, and 1000°C; stress-rupture tests were carried out at 650° and 800°C. The room- and elevated-temperature tensile strength, as well as the stress-rupture life, increased for the same atomic percent in the order palladium, rhodium, ruthenium, osmium. The ductility decreased with increasing concentration or temperature for a given concentration. The results are discussed in terms of solid-solution theory. BOTH solid-solution strengthening and weakening have been observed in alloys. The simple rules which have been suggested to explain alloy strengthening are subject to several exceptions and deviations based on atom size and valency effects. The purpose of the present investigation was to extend the knowledge of the effect of solid-solution alloying on the mechanical properties of several Ni-Pt group metal alloys at room and elevated temperatures. The platinum group metals, osmium, ruthenium, rhodium, and palladium were chosen as the solute elements because of their different valencies and atom sizes. Nickel was chosen as the base material because of the large amount of previous literature available on nickel alloys. EXPERIMENTAL PROCEDURE Grade A Carbonyl nickel powder having the following composition: C, 0.07 pct; Fe, 0.013 pct; Mn, 0.0005 pct; Si, 0.016 pct; Mg, 0.0003 pct; S, 0.003 pct, was purchased from the International Nickel Co. The platinum-group metal powders were purchased from A. D. Mackay Co. The powders were weighed, cone-blended for 4 hr, and vacuum-melted into 1-in.-diam billets, approximately 2 in. long. The ingots were homogenized for 5 hr at 1800°F before being extruded into 1/4-in. rods at 2100°F. The alloy compositions are shown in Table I. Typical impurity values were not significantly different than that of the as-received nickel. All alloys were single phase. The lattice parameter of each alloy after the heat treatment described below is also included in Table I. Each alloy was annealed at 2200°F for 1 hr and air-quenched to comparable grain sizes (ASTM G.S. No. 4-5). The rods were then machined into test samples 0.160-in. diam and 0.750-in. gage length. Tension testing was carried out in an In-stron tension-testing machine at a strain rate of 0.02 in. per in. per min. An extensometer was used to determine the room-temperature yield stress. Stress-rupture testing was carried out in an Arc Weld stress-rupture unit. All testing was performed in air. EXPERIMENTAL RESULTS A) Room-Temperature Mechanical Properties. The 0.2 pct yield stress, ultimate tensile strength, and elongation for all alloys tested at room temperature are plotted as a function of atomic percent solute element in Fig. 1. The ultimate tensile strength for the same atomic percent increases in the order palladium, rhodium, ruthenium, osmium. The yield strength at low concentrations, -0.5 at. pct, increases in the order osmium, palladium, ruthenium, rhodium. At higher concentrations, 3.0 and 10.0 pct, the yield strength increases in the same order as the tensile strength. Both yield strength and tensile strength increase rapidly ini-

Jan 1, 1964

Members Dues Resignations, Suspensions and Expulsions Institute Meetings Board of Director?s Meetings Directors and Officers Duties of Officers Committees Nomination and Election of Officers Publications Divisions, Local Sections, Affiliated Societies Amendments [As REVISED FEBRUARY 21, 19281 ARTICLE I MEMBERS-QUALIFICATIONS AND ELECTION , SEC. 1. The membership of the Institute shall comprise six classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Associates; 6. Rocky Mountain Members. All shall be equally entitled to the privileges of membership, excepting that Junior Associates, and all Members and Associates whose residence shall be outside of the United States of America, Mexico and Canada shall not be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the class of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members.

Jan 1, 1928

By John E. Sherborne, William M. Newton

THE relation between the properties of electric logs and the fluid used in drilling a well is briefly discussed in this paper, and the fact that the resistivity of the drilling mud and its filtrate can appreciably affect such logs is shown. Apparatus was designed and a procedure established to determine the effect of various factors on the resistivity of drilling mud. Five muds commonly employed in California were tested and the following observations were made: I. The effect of raising the temperature from 80°F. to 180°F. is to decrease the resistivity of the mud or filtrate approximately 50 per cent. 2. The resistivity of the mud in most cases closely approximates that of its filtrate. 3. The change in the resistivities of muds caused by the addition of chemical is not the same function of the amount of chemical added for each mud. 4. The effect produced by increased sodium chloride content is to reduce markedly the resistivity of the mud and its filtrate. 5. Weighting materials, such as Baroid and limestone, tend to increase the resistivity of drilling mud. 6. Cement and counteracting reagents reduce mud resistivity.

Jan 1, 1942

CONTENTS PAGE BARTON, D. C.-The Eötvös Torsion Balance Method of mapping Geologic Structure (T. P. No. 50) 1 GEORGE, P. W.-Experiments with Eötvös Torsion Balance in the Tri-State Zinc and Lead District (T. P. No. 65). 15 LANCASTER-JONES, E.-The Computation of Eötvös Gravity Effects (T. P. No.75) HEILAND, C. A.-A Cartographic Correction for the Eötvös Torsion Balance-(T. P. No. 52) 17 SLICHTER; L. B.-Certain Aspects of Magnetic Surveying (T. P. No. 120). . . . 18 WEAVER, W.-Certain Applications of the Surface Potential Method (T. P. No.121) LUNDBERG, H.-Recent Results in Electrical Prospecting for Ore (T. P. No. 98). . 20 HOTCHKISS, W. 0., ROONEY, W. J. and FISHER, J.-Earth-resistivity Measure-ments in the Lake Superior Copper Country (T. P. No. 82) 21 LEONARDON, E. G. and KELLY, S. F.-Some Applications of Potential Methods to Structural Studies (T. P. No. 115) 23 MASON, M.-Geophysical Exploration for Ores (T. P. No. 45) 25 The Eötvös. Torsion Balance Method of Mapping Geologic Structure Discussion of the paper of D. C.. Barton, issued as Technical Publication No. 50 with Mining and, Metallurgy, February, 1928. D. C. BARTON.-The field surveys which I have been privileged to use as illustrations for this paper were done for Mr. DeGolyer's companies and were released through his favor. W. J. MILLARD, Tulsa, Okla.-Has any oil been found by the torsion balance in West Texas? D. C. BARTON.-NO new oilfield has been discovered on the basis of torsion balance work. It has had some part in controlling the policy of certain companies in playing the extension of known oil fields. A number of "T. B." structures have been drilled and dry holes obtained. Of those known to the writer, one apparently was a structural high, one is a broad general high but locally low and probably is a deep-seated structural high, one seems normal although the control is poor, and one was considered structurally low but is now suspected by some geologists of being structurally high. E. L. DEGOLYER, New York, N. Y.-A large gravity structure, generally referred to, I believe, as the Crosby County Structure, has been found in West Texas. This structure is perfectly symmetrical with the arrows all pointing toward a common center, very much like the Nash salt-dome pattern in Dr. Barton's paper (Fig. 9). One of the peculiar things about it, from the standpoint of the gravity high, is that it is so

Jan 1, 1928

By E. Martinez

Samples of chrysocolla, a hydrated copper silicate, from several sources were submitted to differential thermal analysis (DTA) and thermal gravimetric analysis (TGA). Pure samples of chrysocolla are difficult to obtain, but comparison of the thermograms revealed that certain reactions occurred in all the samples and it is believed that these are due to chrysocolla. Endothermic reactions occurred at 50' to 175°C, 350° to 650°C, and 980° to 1100°C each of which caused a weight loss. The first was due to loss of absorbed water, the second to a dehydroxyla-tion, and the last to conversion of cupric oxide to cuprous oxide. In addition, two exotherms were detected at 685° to 695°C and 935° to 950°C. Infrared spectra of heated samples indicated the exotherms were due to changes in the Si-O bonds leading to the formation of cristobalite. The results suggest that thermoanalysis may be a more sensitive and reliable method for detection and identification of chrysocolla than X-ray diffraction, infrared spectroscopy, or optical techniques. The recovery of copper from oxide ores has been the subject of much research in recent years. One of the principal oxide copper minerals is chrysocolla, a hydrated copper silicate. The information available indicates that it has widely varying properties depending on the origin of the sample. Chrysocolla usually is found associated with cuprite, malachite, azurite, and native copper. Most of these other minerals are recoverable by present day flotation practice, but chrysocolla is lost in the tailings.1,2 Reagent combinations that are successful in laboratory chrysocolla flotation with ore from one source have been found to be ineffective with another. 3 The copper segregation process offers an altemative to beneficiation of oxide copper ores.4'5 The process is of particular interest in processing ores that cannot be treated by conventional hydrometal-lurgical methods because of high acid consumption.6 Fuller understanding of the properties of chryso- colla may prove of value in the search for improvements in both the flotation and segregation processes. Chrysocolla samples from Arizona, Nevada, Chile, Australia, and South Africa were studied by differential thermal analysis (DTA) and thermal gravimetric analysis (TGA). In addition, a sample from Miami, Ariz., was submitted to X-ray diffraction, infrared spectrophotometry, and surface area determination. EQUlPMENT Differential thermal analysis (DTA) detects, amplifies, and records exothermic-endothermic reactions occurring in a sample as its temperature is raised at a constant rate, usually 10°C per minute. A unit made by the Robert L. Stone Co. was used in this study. The tests can be run if desired with a gas streaming through the sample. A thermobalance records weight losses or gains in a sample as its temperature is raised at a uniform rate. The gravimetric analyses (TGA) were run on a Chevenard thermobalance converted electronically for graphic recording. A heating rate of 5°C per minute up to 1100°C was used in these tests. A Perkin Elmer Infrared Spectrophotometer, Model 221, was used with sodium chloride optics obtaining IR spectra in the 2 to 15 region. A pressed pellet technique with potassium bromide was used in preparing the samples. DESCRIPTION OF SAMPLES Chrysocolla is found in the oxidation zones of copper deposits commonly associated with malachite, azurite, and limonite. It is described as varying in composition and in color from bluish green to brown or black. Inclusions of other minerals are usual so chemical analysis of chrysocolla samples may be suspect. However, it is considered by many to be a solid solution of CuO, SiO2 and H2O with a general formula of CuO.SiO2.2H2O or 2CuO.2SiO2. 3H20. Chukhrov7 has described a sample from the Urals as CU3,5(OH)2 (A1Si3) O10.nH2O and stated that chrysocolla is a montmorillonite-type mineral. On the basis of X-ray analyses, DTA, and infrared spectra of chrysocolla from the Inspiration Mine, Ariz., Sun8 concluded that there was no substantial evidence to classify it as a montmorillonite mineral. Chrysocolla samples from many sources throughout the world were used in this investigation. The following is a brief description of each:

Jan 1, 1963

By W. R. Toeplitz

Probably a more descriptive title would be "Much Ado About Nothing." By "nothing," of course, I refer to the porosity which is the main feature of this type of bearing. Porosity has a decided effect on the manufacturing techniques, the structure and physical properties, the oil content, and on the installation and service of oil-retaining porous bronze bearings. A simple curve can be drawn by plotting specific gravity along the abscissa and percentage of porosity by volume on the ordinate. A bronze composition, analyzing 89 Per cent copper, 9.75 Per cent tin, and 1.25 per cent graphite, has an absolute solid specific gravity of 8.5. At this specific gravity, of course, occurs the point of zero porosity. Conversely, at loo per cent porosity, the specific gravity is zero. A similar curve can be drawn for bearings impregnated with oil; the only change being that the specific gravity at loo per cent oil will be 0.89 if we assume that that is the specific gravity of the lubricant. The curve is useful in determining the oil content by volume for any specific gravity. The normal range of oil content for porous bronze bearings of this composition is from 35 to 16 per cent, which is in the specific gravity range of from 5.8 to 7.3. In addition to the amount of porosity, the type of porosity is important. The first consideration here is that the porosity must be intercommunicating. This can be determined by a number of simple tests. The first method, which is very accurate, is to extract the oil in the bearing by cycling

Jan 1, 1945

By Donald E. Grimes

In conjunction with Inland Steel&apos;s development of lead-bearing steels possessing improved machin-ability because of tellurium and/or selenium additions, it was decided to determine liquidus and solidus temperatures in the Pb-PbTe-PbSe sub-ternary system. With the exception of alloys in the PbTe-PbSe system, it is believed that no previous study of this subternary has been performed. Thermal analysis was employed in a general survey of the subternary. In addition to PbTe, PbSe, and pure lead, ten ternary compositions were selected at intervals of ten at. pct. Sixty-gram alloys were prepared by sealing an appropriate mixture of the elements in quartz crucibles with a central thermocouple-well under a vacuum of less than 10 p. All three elements were 99.999+ pct pure with only trace impurities detected by spectroscopic examination. After the alloys had been heated at least 20°C above the liquidus in a Kanthal furnace, cooling and heating curves were obtained. Two or more cooling curves were employed both for the determination of each alloy liquidus and for the solidus of those al- loys containing greater than 50 at. pct Pb. Cooling rates were 0.5° to 3.5°C per min during the 5 min immediately prior to the start or end of solidification. For those ternary alloys containing 50 at. pct Pb, the solidus was determined from heating curves. Temperatures were measured with a Pt/Pt-10 pct Rh thermocouple which was calibrated in the same apparatus against the freezing points of zinc (A. D. MacKay—99.999 pct), antimony (A. D. MacKay-99.999 pct), and copper (ASARCO—99.999+ pct) both before and after the experimentation. The only interruptions in the continuous strip-chart recording of the temperature occurred for brief periods at significant points of interest when direct readings were made with a Rubicon Type B potentiometer sensitive to * 1 µv. The average liquidus and solidus temperatures obtained in this investigation are listed in Table I together with probable errors based on the accuracy of the thermocouple calibration and the reproduci-bility of the data. No chemical analyses of the alloys were performed because the synthetic or as-charged compositions were felt to be reliable. The melting points obtained for PbTe (924.7° ± 0.7°C) and PbSe (1084.0° ± 0.6°C) compare favorably with recent findings of other investigators.&apos;-&apos; As indicated in Table I, both the liquidus and solidus temperatures increase as selenium replaces tellurium for a constant atomic percent lead. As a result, the ternary liquidus and solidus temperatures for a given percent lead lie between the corresponding binary temperatures published in the literature. It should be noted that those ternary alloys containing 50 at. pct Pb exhibit a relatively narrow liquid-plus-solid region (<80°C) when compared with alloys containing greater than 50 at. pct Pb. Alloys with 60, 70, or 80 at. pct Pb not only have a much wider liquid-plus-solid region (>500°C) but also exhibit considerably lower and approximately constant solidus temperatures which thus form a virtually isothermal solidus "plane" slightly below the melting point of pure lead (327.3°C). For these alloys

Jan 1, 1965

By D. W. Rudd, D. W. Vose, J. B. Vetrano

In an earlier paper the permeability character of Mo-0.5 pct Ti to hydrogen was described.&apos; It was shown that this alloy is a more effective barrier to the passage of hydrogen than previously studied systems, i.e., copper,2 nickel,3 and several stainless steels.4 The permeability of Hastelloy B to hydrogen was investigated as a material having promising high-temperature structural properties which might have a low permeability to hydrogen. The general theory of permeation has been previously discussed,&apos; and here only a summary of the more important results are given. It is found that except for very thin membranes, at low temperature, permeation of a gas through a metal barrier is determined by the rate of diffusion of the gas through the crystal lattice of the specimen, and that for hydrogen and the common diatomic gases, this passage involves dissociated particles as the diffusing species. The rate of permeation for hydrogen is therefore proportional to the square root of the pressure. It has also been found that the rate of permeation is inversely proportional to the thickness of the barrier. The apparatus used in this investigation was fundamentally the same as that employed in previous studies,&apos; except that several simplifications result in the case of Hastelloy, since oxidation at the temperatures investigated is no longer a problem and welding of the specimen is relatively easy. A cross section of the membrane assembly is shown in Fig. 1. When finished, the assembly is about 5 in. long. The wall thickness is about 6 times the membrane thickness. The membrane (A) can be maintained at

Jan 1, 1963

By Edward Keller

Under the title, Labor-Saving Appliances in the Works-Laboratory, I published a paper1 in which mas described how multi-manipulations in a works-laboratory and in the furnace-room of an assay-laboratory, can be condensed into single manipulations by applying the proper mechanical devices. For example, I now deposit ill, or withdraw from, a muffle a set of 48 cupels as one unit. The front row (8) of these are blanks or heaters; the other 40, when they have attained the proper temperature in the muffle, are charged simultaneously with the 40 lead-buttons. Three manipulations here accomplish an operation which by the generally customary method requires 136, and this number is only limited by the size of muffle and cnpels. This operation is an enlargement of what I have already described in my former paper, and Fig. 1 shows the improved implements. In the paper referred to I described a gold-silver bead parting-bath, which is the last of the devices used in regular sequence in practice. This bath mas designated as being convenient, but mas not a labor-saver properly. Fig. 2 of the present paper shows a new device. Instead of the original tray, there are now sectional holders for the test-tubes, each having a wooden handle on either end, so that the holders ma?-be removed from the boiling bath, and the acid or water poured oE from each set of tubes (in this case, 7) without waiting to cool. The tubes, held in place by clutches, as shown in Pig. 3, rest in holes in the base-strip, having a smaller diameter than the tubes. Each holder is stamped at either end with a number, so that the bath becomes further useful by permitting several men to use it at the same time without interference. Apart from the handles, the holders are made of sheet-copper.

Jan 1, 1911

By Y. L. Yao

The solubility limit of oxygeu in a titanionn at 850°C has been determined by magnetic measurements as 12.5 + 0.5 pct (29.0—30,9 at. pct). Also in the susceptibility-co~centmtion curve, there is n distinct but not sharp maximum at 19.0 * 0.5 z~t pet (40.5--42.1 at. pct), which indicates the presence of the 6 phase. The magnetic susceptibilities of the alloys of the titanium-oxygen system were determined byEhrlich in 1939.&apos; is alloys were prepared by sintiring mixtures of titanium and its oxide at high temperatures. On the titanium-rich side, despite the fact that the alloy compositions he measured crossed two phase boundaries, the limited results obtained

Jan 1, 1960

By H. W. Maynor, C. J. McHargue

DURING the course of an investigation of materials suitable for use as thermocouples at elevated temperatures by one of the authors, several nlolybdenum-rhenium alloys were prepared. Micrographs of an annealed alloy containing 25 pct Re (intended concentration; analysis not obtained) showed a number of twins, Fig. 1, suggesting a face-centered cubic structure. This note reports the structure and recrystallized wire texture of an alloy containing 25 wt pct Re. Alloys were prepared from 99.9 pct Mo (Fansteel Metallurgical Corp.) and rhenium obtained from the University of Tennessee (purity unreported). Powders were combined and briquetted at 56,000 psi and sintering was carried out at 2400°C for 5 hr in vacuum. Ingots so prepared were swaged at 982.2" to 1037.8oC into wires 0.036 in. diameter, a reduction in diameter of 85.6 pct. These wires were vacuum-annealed 1 hr at 2000°C. A North American Philips 114.59 mm powder camera and nickel-filtered copper radiation were used for structure determination. For the texture determination a Laue-type camera was used with zirconium-filtered molybdenum radiation and, because of the high background, aluminum foil was mounted next to the film. Exposures were taken with the wire perpendicular to the X-ray beam and tilted by 10". It was found that the X-ray pattern could be indexed on the basis of a face-centered cubic structure. Because of difficulties associated with obtaining a good X-ray pattern for this material, accurate parameter determinations were not made. An indicated parameter value of 3.70A was obtained. The X-ray data are given in Table I. The annealed wire texture was observed to be a sharp [111] texture. The spread about this fiber axis was k8" at the surface of the 0.036 in. wire. The annealed wire textures of aluminum have been reported as retention of the [Ill] deformation texture for anneals below 500°C and a new [1121 texture for anneals above 600°C.1 In copper wires, with a [Ill] plus [loo] deformation texture, results indicate a retention of this texture for annealing at lower temperatures and new components or the disappearance of components for annealing at higher temperatures.&apos; The presence of the strong [I111 texture in the molybdenum-rhenium alloy after a 2000 °C anneal suggests that the deformation texture was the same. Acknowledgment The wires used in this study were prepared and heat-treated at the Institute for Atomic Research, and Ames Laboratory, Iowa State College, and the authors wish to express their thanks to the Institute for allowing the use of the material and permission to publish the results.

Jan 1, 1954

By F. R. Brotzen, A. R. Troiano, E. L. Harmon

Precipitation processes leading to drastic property changes are a frequent occurrence in titanium alloys containing large amounts of the retained high temperature P phase. In order to establish the kinetics and nature of these precipitation processes, a series of Ti-V alloys was studied. Time-temperature-transformation diqgrams were obtained for 12.5 and 15 pct V-Ti alloys. These diagrams consisted of two intersecting C-shaped curves: one in the high temperature region for the euilibrium transformation P +u+P, and another at lower temperatures depicting the formation of the meta-stable transition phase, o. Presence of the transition phase retarded the precipitation of the equilibrium a phase. Deformation of retained P resulted in the formation of the o phase. Reversion and retrogression phenomena of the transition phase were observed. A negative temperature coefficient of resistance was found in quenched alloys containing from 15 to 20 pct V. CERTAIN titanium-base alloys can be heat treated to produce appreciable changes in properties. For example, remarkably high hardness values may be obtained by aging or isothermal quenching treatments. Most of the information available to date on the hardening of titanium-base alloys has been systematized recently in an article by L. D. Jaffe.&apos; It was pointed out by that author that the hardening was the result of the decomposition of the retained j3 phase to the equilibrium constituents, a and p, and that this decomposition had many of the characteristics of an age-hardening reaction. Recent work by Frost et al.&apos; 3 has contributed much to the fundamental understanding of the hardening mechanism in titanium-base systems. These authors established the presence of a transition phase in the transformation from j3 to a + j3, which they designated o. The transition phase, in their opinion, was at least partially responsible for the hardening and embrittling effects which accompanied low temperature aging. The present investigation of the mechanism and kinetics of the hardening reaction was carried out for the Ti-V system. Ti-V alloys were ideally suited for a study of the decomposition of j3, since age hardening was known to occur readily in this system." Moreover, no intermetallic compounds occur in this system, Fig. 1, thus simplifying the interpretation of the results. Material and Procedure Alloys containing 12.5 and 15 pct V were prepared by Battelle Memorial Institute from iodide titanium furnished by Watertown Arsenal and vanadium of 99.8 pct purity. Ingots of 8 Ib each were prepared by arc melting in an inert atmosphere with a tungsten electrode and water-cooled copper crucible. Each of the ingots was melted once, forged at 1600°, and rolled at 1400°F. Following this, the ingots were remelted, forged, and then rolled to % in. sq bars, which were subsequently grit blasted, pickled, and wire brushed. Another set of alloys containing nominally 17.5 and 20 pct V was produced by the Research Div., New York University. These alloys were arc melted in an inert atmosphere in lots of 20 g each. Heat-Treating Procedure: Whenever feasible, specimens were heat treated in high vacuum resistance furnaces at pressures below 5x10." mm of Hg. Aging and isothermal quenching treatments were generally carried out in salt baths. Specimens were not attacked by the salt, provided the tempera-

Jan 1, 1956

By David R. Mitchell

The mineral pyrite (or marcasite) occurs in coal beds as balls, lenses, veinlets and bands. Several million tons are wasted annually on the refuse dumps from coal mining and coal-preparation activities. Sporadic attempts have been made in the United States to recover this pyrite for manufacture of sulphuric acid but only a few plants have succeeded in recovering it on a commercial scale. Several chemical companies in the East became concerned about supplies of pyrite early in 1943, but by late summer of that year the situation had eased. If for no other reason than national security and self-sufficiency during wartime, methods of recovering pyrite from coal-mine refuse should be worked out and made available to coal-mine operators who are potential producers of pyrite. Eastern sulphuric-acid plants are particularly likely to have their sources of raw material blocked by war conditions, so that special studies to determine where supplies of pyrite can be obtained for these plants from inland sources are desirable. Davis&apos;s1 summarization of conditions during World War I gives the following facts: During those years, the shortage of pyrite became acute. Shipments of hand-picked pyrite were made from a number of coal mines in Illinois, Indiana, western Kentucky, Ohio and Pennsylvania. A mechanical concentrating plant for sepa- rating pyrite from picking-table refuse was built at Danville, Ill., and operated for several years, and a small pyrite-concen-trating plant treating washery refuse near Gillespie, Ill., operated for several months in 1918. The Consolidation Coal Co. of Fairmont, W. Va., constructed and operated a sulphuric-acid plant using pyrite recovered from coal-mine refuse. The U. S. Bureau of Mines during 1917-1919 made a comprehensive survey of pyrite-production possibilities from coal mines and estimated that there was a potential yearly production of 435.000 tons from Ohio and Pennsylvania and 928,000 tons from Kansas, Missouri, Iowa, Illinois, and Indiana mines. This estimate included only mines that could produce one per cent or more of their coal production as pyrite containing a minimum of 40 per cent sulphur. PyRite Production According to the Minerals Yearbook,2 approximately 660,000 long tons of pyrite was produced in the United States in 1941, with an average sulphur content of 42 per cent. The average value f.o.b. mines was $3.09 per long ton. Spanish pyrite, 48 per cent sulphur minimum, was quoted at 12 cents a unit c.i.f. U. S. ports, equal to $5.76 a ton for shipments of minimum sulphur content. Most of the pyrite produced in the United States is obtained as a by-product in the dressing of copper and zinc ores. Metal mines in the East making pyrite concentrate for the market or use in company-operated sulphuric-acid plants

Jan 1, 1944

By David R. Mitchell

The mineral pyrite (or marcasite) occurs in coal beds as balls, lenses, veinlets and bands. Several million tons are wasted annually on the refuse dumps from coal mining and coal-preparation activities. Sporadic attempts have been made in the United States to recover this pyrite for manufacture of sulphuric acid but only a few plants have succeeded in recovering it on a commercial scale. Several chemical companies in the East became concerned about supplies of pyrite early in 1943, but by late summer of that year the situation had eased. If for no other reason than national security and self-sufficiency during wartime, methods of recovering pyrite from coal-mine refuse should be worked out and made available to coal-mine operators who are potential producers of pyrite. Eastern sulphuric-acid plants are particularly likely to have their sources of raw material blocked by war conditions, so that special studies to determine where supplies of pyrite can be obtained for these plants from inland sources are desirable. Davis&apos;s1 summarization of conditions during World War I gives the following facts: During those years, the shortage of pyrite became acute. Shipments of hand-picked pyrite were made from a number of coal mines in Illinois, Indiana, western Kentucky, Ohio and Pennsylvania. A mechanical concentrating plant for sepa- rating pyrite from picking-table refuse was built at Danville, Ill., and operated for several years, and a small pyrite-concen-trating plant treating washery refuse near Gillespie, Ill., operated for several months in 1918. The Consolidation Coal Co. of Fairmont, W. Va., constructed and operated a sulphuric-acid plant using pyrite recovered from coal-mine refuse. The U. S. Bureau of Mines during 1917-1919 made a comprehensive survey of pyrite-production possibilities from coal mines and estimated that there was a potential yearly production of 435.000 tons from Ohio and Pennsylvania and 928,000 tons from Kansas, Missouri, Iowa, Illinois, and Indiana mines. This estimate included only mines that could produce one per cent or more of their coal production as pyrite containing a minimum of 40 per cent sulphur. PyRite Production According to the Minerals Yearbook,2 approximately 660,000 long tons of pyrite was produced in the United States in 1941, with an average sulphur content of 42 per cent. The average value f.o.b. mines was $3.09 per long ton. Spanish pyrite, 48 per cent sulphur minimum, was quoted at 12 cents a unit c.i.f. U. S. ports, equal to $5.76 a ton for shipments of minimum sulphur content. Most of the pyrite produced in the United States is obtained as a by-product in the dressing of copper and zinc ores. Metal mines in the East making pyrite concentrate for the market or use in company-operated sulphuric-acid plants

Jan 1, 1944

By David R. Mitchell

THE mineral pyrite (or marcasite) occurs in coal beds as balls, lenses, veinlets and bands. Several million tons are wasted annually on the refuse dumps from coal mining and coal-preparation activities. Sporadic attempts have been made in the United States to recover this pyrite for manufacture of sulphuric acid but only a few plants have succeeded in recovering it on a commercial scale. Several chemical companies in the East became concerned about supplies of pyrite early in 1943, but by late summer of that year the situation had eased. If for no other reason than national security and self-sufficiency during war-time, methods of recovering pyrite from coal-mine refuse should be worked out and made available to coal-mine operators who are potential producers of pyrite. Eastern sulphuric-acid plants are particularly likely to have their sources of raw material blocked by war conditions, so that special studies to determine where supplies of pyrite can be obtained for these plants from inland sources are desirable. Davis&apos;s1 summarization of conditions during World War I gives the following facts: During those years, the shortage of pyrite became acute. Shipments of hand-picked pyrite were made from a number of coal mines in Illinois, Indiana, western Kentucky, Ohio and Pennsylvania. A mechanical concentrating plant for separating pyrite from picking-table refuse was built at Danville, Ill., and operated for several years, and a small pyrite-concentrating plant treating washery refuse near Gillespie, Ill., operated for several months in 1918. The Consolidation Coal Co. of Fairmont, W. Va., constructed and operated a sulphuric-acid plant using pyrite recovered from coal-mine refuse. The U. S. Bureau of Mines during 1917-1919 made a comprehensive survey of pyrite-production possibilities from coal mines and estimated that there was a potential yearly production of 435,000 tons from Ohio and Pennsylvania and 928,000 tons from Kansas, Missouri, Iowa, Illinois, and Indiana mines. This estimate included only mines that could produce one per cent or more of their coal production as pyrite containing a minimum of 40 per cent sulphur. PYRITE PRODUCTION According to the Minerals Yearbook,2 approximately 660,000 long tons of pyrite was produced in the United States in 1941, with an average sulphur content of 42 per cent. The average value f.o.b. mines was $3.09 per long ton. Spanish pyrite, 48 per cent sulphur minimum, was quoted at 12 cents a unit c.i.f. U. S. ports, equal to $5.76 a ton for shipments of minimum sulphur content. Most of the pyrite produced in the United States is obtained as a by-product in the dressing of copper and zinc ores. Metal mines in the East making pyrite concentrate for the market or use in company-operated sulphuric-acid plants

Jan 1, 1944

By B. W. Levinger

THE system Ti-CI- has been studied by several investigators." &apos; Though titanium and chromium are completely miscible at high temperatures, an intermediate phase of the approximate atomic proportions TiCr, has been identified at various compositions between 60 and 68 wt pct Cr. The structure of this phase was established as the cubic C15 (MgCu2) type with 24 atoms per unit cell and a lattice parameter 6.929 kX.2 During a study of the ternary system, Ti-Mo-Cr,5 the existence of a high temperature modification of the TiCr, phase was discovered. In a series of alloys annealed at 1300°C and containing from 60 to 70 wt pct Cr and 5 pct Mo, a new phase was present which did not correspond to either ß solid solution or TiCr,. By trial, the new phase was identified to be of the hexagonal C14 (MgZn2) structure with 12 atoms per unit cell. Further work showed that the hexagonal structure was. in fact, also present in binary Ti-Cr alloys quenched from high temperatures. To make the identification more certain, the intensities of the various reflections were calculated assuming a composition TiCr2 and C14 structure. Table I lists reflection planes, interplanar distances, calculated intensities, and a comparison of these values with the lines of a binary Ti-Cr alloy (66 pct Cr) annealed for 20 min at 1385°C and water quenched. Since high angle lines were more diffuse, the correspondence between visually observed and calculated intensities was not as good at these angles. Lattice parameters were computed to be a = 4.922 kX, c = 7.945, c/a :- 1.614. The corresponding interatomic distances are: titanium to titanium distance, 3.00:, kx, chromium to chromium distance, 2.43, kX, titanium to chromium distance, 2.88,, kX. These compare to 3.00, 2.45, and 2.87 kX in the cubic phase, respectively.&apos; The atomic positions in the C14 structure are as follows: Titanium 1/3, 2/3, Z; 1/3, 2/3, 1/2: 2/3, 1/3, i; 2/3, 1/3, (1/2-z); Chromium 0, 0, 0: 0, 0, 1/2; 2x, 2, 1/4; 232, x, %; X, 22, 1/4; X, 2x, 3/4; x. x, 1/4; x, x, 3/4; The values of x and z were calculated for the alloy mentioned and found as follows: z — 0.061, x = 0.165. The values assumed in the intensity calculations were those for an ideal close-packed lattice or z = 1/16, x = 1/6. Work in the Ti-Mo-Cr system indicates that y2 the hexagonal modification of TiCr2, is the stable phase above 1300°C, while y1 with the cubic structure is stable below 1000°C. X-ray examination of a number of alloys annealed at intermediate temperatures showed that the hexagonal and cubic phases can coexist. Alloys quenched from 1000°C and annealed at 1100" and 1200°C showed small amounts of y2 at the higher temperature. A considerable amount of y, seemed present, however, in cast alloys annealed at 1100°C. It further appears that there is a small but definite solubility range for both phases in the ternary system. Acknowledgment The results of this paper represent work carried out in conjunction with a project sponsored by Watertown Arsenal, Contract No. DA-11-022-ORD-272. References &apos;M. K. McQuillan: Journal Inst. Metals (1951) 79, p. 379. 2 P. Duwez and J. L. Taylor: Trans. ASM (1952) 44, p. 495. W. J. Van Thyne,. H.. D. Kessler, and M. Hansen: Trans. ASM (1952) 44, p. 974. 1 F. B. Cuff, N. J. Grant, and C. F. Floe: Trans. AIME (1952) 194, p. 848; Journal of Metals (August 1952). Unpublished Research, Armour Research Foundation. "H. J. Wallbaum: Ztsch. Krist. 103, p. 391.

Jan 1, 1954

By Charles S. Barrett, F. W. Steadman

DEFORMATION bands of surprising regularity are found in large-grained polycrystalline copper after cold-rolling (Fig. I). Individual bands frequently are large enough to permit a determination of their orientation by means of etch pits and an optical goniometer. Measurements have been made on 21 areas in seven different grains, and these, combined with X-ray studies of nine single crystals that had been cold-rolled after mounting in a polycrystal-line block, have contributed to a better understanding of the preferred orientations in rolled copper just as similar studies have for rolled iron&apos; and brass.2.3 Particular attention was given to determining orientations that are stable during rolling and to the manner of fragmentation and rotation of unstable grains. The possible role of twinning was also carefully investigated. The texture of polycrystalline copper after cold-rolling is well established by the pole figures that have been plotted by Schmid and Staffelbach,4 Iweronowa and Schdanow,5 and Brick and Williamson,3 all of which are in substantial agreement. There has been some divergence in the list of individual "ideal" orientations that have been used to describe the texture by these observers and others,6 although the orientation (110) [112]-that is, (110) parallel to the rolling plane and [112] parallel to the rolling direction-is generally recognized as the most prominent orientation and (I12) [111] one of the lesser orientations. Other orientations have been given by some observers as (236) [533], (100) [001], and (I 10) [001]. The texture of copper has also been described as (135) [533].6.1 The sum of these orientations provides a reasonable approximation to the complete pole figure, but it does not follow that these specific orientations are necessarily of fundamental significance, for the choice of indices is arbitrary, within limits. Furthermore, a detailed investigation of the ideal orientations in cold-rolled iron discloses continuous ranges of equally favored positions rather than definite positions of high stability,1 and similarly Brick&apos;s observations in a single crystal of a brass2 suggest that all orientations in the range between (110) [113] and (110) [117] are about equally stable. MATERIALS AND METHODS The material used was vacuum-cast electrolytic copper kindly supplied by L. L. Wyman, of the General Electric Co.* Slices 1/2 in. thick and 2 1/2 in. square, cut from the ingot, were rolled with 50 per cent reduction per pass to final thicknesses between 0.02 and 0.04 in., and etched to develop cube-face etch pits suitable for goniometric work.8 The etch was light on some strips and deep in others.

Jan 1, 1942